Method of producing powder composed of precisely spherical particles

ABSTRACT

Method for producing a synthetic resin powder composed of precisely spherical particles wherein a solution material is prepared by dissolving a synthetic resin in a solvent, spraying the solution in the presence of a separation agent, removing the separation agent from the sprayed material after recovery, and drying the resultant product.

United States Patent 1 [111 3,887,668 Honjo *June 3, 1975 [5 METHOD OF PRODUCING POWDER [58] Field of Search 264/13, 14

COMPOSED OF PRECISELY SPHERICAL PARTICLES [56] References Cited Inventor: Kazuo Honjo, Nishinomiya, l-lyogo,

Japan Assignee: Ideki Co., Ltd., Japan Notice: The portion of the term of this patent subsequent to June 12, 1990, has been disclaimed.

Filed: May 3, 1973 Appl. No.: 356,951

Related U.S. Application Data Continuation-in-part of Ser. No. 95,403, Dec. 4, 1970, Pat. No. 3,739,049.

U.S. Cl. 264/14 Int. Cl B0lj 2/06 UNITED STATES PATENTS 3,739,049 6/1973 Honjo 264/14 Primary ExaminerRobert F. White Assistant ExaminerJ. R. Hall Attorney, Agent, or FirmGeorge B. Oujevolk [5 7] ABSTRACT 8 Claims, 2 Drawing Figures PATENTEDJUH3 1975 METHOD OF PRODUCING POWDER COMPOSED OF PRECISELY SPHERICAL PARTICLES This application is a continuation-in-part application of Ser. No. 95,403 filed Dec. 4, 1970, now U.S. Pat. No. 3,739,049.

BACKGROUND OF THE INVENTION The present invention relates to a method for producing a powder composed of precisely spherical particles, more particularly, to a method for producing a synthetic resin powder composed of precisely spherical particles to be used, for instance, for powder coating.

In recent years, the powder coating method of apply ing a synthetic resin in the form of powder to a surface to be coated has come into extensive use because of its outstanding advantages. Presently, synthetic resin powder to be used for powder coating is produced either by a chemical method in which powder is obtained by polymerization or by a mechanical method wherein a resin in the form of pellets or in some other solid form is pulverized. However, the former is not a method which is practiced exclusively for use with powder coating, but part of the amount of powder thereby produced is merely utilized for powder coating, so that a powder of an optimum particle size cannot be obtained. The former method therefore has inevitable disadvantages of high cost and difficulty to obtain particles in the form of true spheres. On the other hand, the latter has other disadvantages that particles produced are irregular in shape, some being fluffy or threadlike. and that the particle size varies over a wide range of distribution. In order to insure high fluidity of the powder for powder coating so as to obtain a uniformly smooth surface, it is necessary to use a synthetic resin powder composed of precisely spherical particles which are uniform in particle size.

SUMMARY OF THE INVENTION The present invention provides a method for producing a particulate synthetic resin in the form of true spheres which meets the foregoing requirements and generally comprises the steps of preparing a solution by dissolving a synthetic resin in a solvent, spraying the so lution in the presence of a separation agent, removing the separation agent from the sprayed material after re covery, and drying the resultant substance.

In accordance with the method of this invention, powder of a desired particle size can be obtained by varying the foregoing production conditions. Because of the spraying operation, exactly spherical particles of the same size can be obtained efficiently. In the case where metal powder such as aluminum, brass, stainless steel or the like, ceramic material or sand is added to the liquid material, particles of such material will be put together and coated with synthetic resin, with the result that they look beautiful because they can be seen through the coating. The synthetic resin powder obtained by the method of this invention insures smooth surface free of irregularity when used for powder coating.

The present invention will be described in greater detail with reference to the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a front view in vertical section showing an apparatus for producing a synthetic resin powder composed of precisely spherical particles in accordance with the method of this invention; and.

FIG. 2 is a side elevation in section taken along the line 2 2 in FIG. 1.

DESCRIPTION OF THE PREFERRED EMBODIMENTS Referring to FIG. 1, there is shown a shallow tank 2 which has legs 1. Mounted on the tank 2 is a tank 4 which is in the form of an inverted U-shape in section and slightly smaller than the tank 2 in size, the tank 4 being provided with an opening 3. Thus, a chamber 5 is formed. Disposed inside the tank 4 at the center of the opposite side walls thereof are sets of annular sprayers 8 for a separation agent and sprayers 6 for a solution 9 disposed at the center of the annular sprayers 8, each of the sprayers 8 being provided with sev eral nozzles 7. In order to eject the solution 9 from the sprayer 6 under pneumatic pressure, the sprayer 6 is provided with a feed pipe 10 for the solution and another feed pipe 11 for compressed air. On the inside of the upper wall of the tank 4, there is a dispersing pipe 13 for a separation agent which extends along the whole side wall, i.e., along the inside upper end of the peripheral wall of the tank 4. The pipe 13 has a plurality of nozzles 12. The sprayer 8 and the dispersing pipe 13 communicate with the same feed pipe 14 for supplying the separation agent, so that the same separation agent 15 is discharged from the sprayer 8 and the pipe 13 under hydraulic pressure.

A tank 17 provided with short legs 16 is positioned beside and below the tank 2, and an outlet pipe 18 extends from the side wall of the tank 2 downward into the tank 17 so as to flow a mixture 19 of powder and the separation agent, received by the tank 2, into the tank 17. Fixed to the tank 17 at its side wall is a drain pipe 21 carrying a cock 20.

The solution 9 is obtained by dissolving a synthetic resin in a solvent. When desired, a pigment may be added to the solution. Where necessary, a plasticizer or a blowing agent may further be added. Any synthetic resin is applicable insofar as the resin can be dissolved in a solvent with or without heating. For instance, conveniently employable are epoxy resin, acrylic resin, alkyd resin, cellulose derivatives, polyvinyl acetal, and copolymer of vinyl chloride and vinyl acetate, since these are soluble in a solvent without heating. Further, polyethylene, nylon and vinyl chloride which are readily soluble in a solvent by heating may also be used.

Through the feed pipes 10, the solution is sent to the sprayers 6, from which it is sprayed into the chamber 5 under the pressure of the air supplied by the feed pipes 11. Since the solution 9 is ejected from the sprayers 6, it is required that the viscosity of the solution be adjusted to 5 to 200 centistokes. The pressure of the compressed air should be at least 4kg/cm so that the solution 9 may be dispersed in the form of spray when discharged from the sprayers 6.

When the liquid solution is ejected into the chamber 5, the liquid separation agent 15 is sprayed from the sprayers 8 and the dispersing pipe 13 simultaneously therewith. The spraying force of the separation agent is less than that of the sprayed solution. i.e., if the compressed air pressure for the solution is 4kg/cm the separation agent should be about 3kg/cm Employable as the separation agent are water, preferably deionized water. hot water having a temperature of about l60F, petroleum, solvent naphtha. mineral turpentine. Economically, however, water is the most preferable.

The solution 9 ejected from the sprayer 6 is dispersed in the form of spray, i.e., in the form of true sphere or particles resembling ture sphere. The solvent is volatilized before the powder falls into the tank 2. Even if the solution 9 is reduced to powder upon spraying, the resultant minute particles tend to get together while falling downward, but the separation agent 15 discharged from the nozzles 7 of the sprayers 8 serves to prevent such tendency. Thus, the separation agent 15 keeps contact with the atomized solution 9 is greater than that of the separation agent 15, the latter is attracted to the former, thus serving to separate the respective particles of the powder which are still sticky while they drop into the tank 2 in which a small amount of separation agent is placed in advance.

On the other hand, the separation agent 15 sprayed from the annular dispersing pipe 13 and flows down continuously along the inner face of peripheral wall of the tank 4 so that the splashed powder which is still sticky is prevented from sticking to the inner face of the tank 4.

The mixture 19 of the powder and separation agent received by the tank 2 is led into the tank 17 through the outlet pipe 18 and. when a predetermined amount is recovered, the cock 20 is opened to transfer the mixture to a centrifugal separator (not shown) by way of the drain pipe 21. After the separation agent has been removed by the centrifugal separator, the resultant substance is dried and a finished product of powder comprising precisely spherical particles is obtained. The particle size of the powder is about 5 to about 200 ,u. If it is desired to reduce the particle size, the viscosity of the liquid material 9 may be lowered or spraying pressure may be reduced.

Although the drawing shows sets of the sprayer 6 for solution and sprayers 8 for separation agent are fixed to the opposite side walls of the tank 4 in facing relationship, the number of the set may be varied as desired. While the separation agent 15 is so sprayed as to center around the spray of solution 9, the separation agent 15 may be ejected in such direction as to intersect the spray of solution 9 at right angles or at some other angle. The same powder as above will be obtained, if the tank 2 is sufficiently filled with the separation agent 15 in advance and the nozzles of the sprayer for solution are put into the separation agent 15 to eject the solution therein. In this case, the sprayer for the separation agent will of course be dispensed with. However, the ejection pressure of the solution sprayer should preferably be greater than is the case with ejection in the air, the requisite pressure being 4kg/cm or over e.g., 6.5 kg/cm. Further, in the simplest mode of operation, the feed pipe 11 for compressed air may be used as the pipe for feeding the separation agent, into which steam may be supplied. in accordance with this method, the solution is sprayed under the steam pressure, while the steam serves to effect separation. Provision ofa heater on the feed pipe 10 for the solution at the intermediate position thereof facilitates flow of the solution 9 for easier spraying operation.

EXAMPLE 1 A solution formed by dissolving a synthetic resin in a volatile organic liquid solvent was prepared by dissolving l,000 g of 6,!0 nylon in 15 kg of phenol. 200 liters of deionized water serving as a separation agent and containing g or an addition product of nonylphenol ethylene oxide, a nonionic activator, was prepared separately. Employing the illustrated apparatus, the solution was sprayed in the presence of the separation agent, and after recovery, the separation agent was removed from the sprayed substance. By drying the resultant product, 985 g of a powder material to be used as an additive for face powder and composed of precisely spherical particles 5 to 43 a in size was obtained.

EXAMPLE 2 A solution formed by dissolving a synthetic resin in a volatile organic liquid solvent was prepared by mixing together at room temperature l00 g of epoxy resin, 50 g of titanium white, serving as coloring agent, 8 g of dicyandiamide, hardner, and 150 g of methyl ethyl ketone, solvent. 2 liters of solvent naphtha was prepared as a separation agent. Employing an apparatus as illustrated, the solution was sprayed in the presence of the separation agent, and after recovery the separation agent was removed from the sprayed substance. By drying the resultant product, 160 g of a powder of the above solutes composed of precisely spherical particles 10 to 105 ,u in size was obtained.

EXAMPLE 3 A similar solution was prepared by emulsifying g of epoxy resin, l0 g of polyamide and 260 g of tetrahydrofuran in 3 liters of deionized water containing an addition product of nonylphenol ethylene oxide. 2 liters of deionized water was separately prepared as a separation agent. The solution was sprayed in the presence of the separation agent by an apparatus as illustrated and, after recovery, the separation agent was removed from the sprayed substance. By drying the resultant product, g of a powder material composed of precisely spherical particles 0.5 to 3 ,u. in size was obtained.

Example 4 Solution:

Epoxy resin Dicyandiamide Titanium white Tetrahydrofuran Separation agent:

Water Polyoxyethylene alkylether Product:

Epoxy resin powder composed of precisely spherical particles 5 to 44 ,u. in particl size, the powder having apparent specific gravity 0.7 and yield 95 g.

While spraying the separation agent at a pressure of 3 kg/cm the solution was sprayed at a pressure of 7 kg/cm providing with compressed air and both were brought into contact with each other by employing the apparatus shown in the drawing.

Example 5 Solution:

Thermoplastic polyester resin I000 g Exam le,5- Contin ue d y 4 p -Wh1l'e spraying the separation agent at a pressure of Methylethylketon 5000 g WWW- C5t 3 kg/cmthe solution was sprayed at a pressure of 4 sepuwtiyn g l'tg/cm' providing with-compressed air and both were aer t W. polygxyethylem mmylphemle I y 5 br ught mto contact with each other by employing the Product: apparatus shown in the drawing.

Thermoplastic polyester resin powder of r 1 precisely spherical particles with excellent Example 9 fluidity and 15p. inihighest frequency size, the powder having apparent specific grayity" 0.35 and yield 955g 10 Solution:

' Polystyrene 1000 g I V 'Methylethylketone 4000 g 4 I Viscosity: 200 cSt Whlle2spray1ng the separatlonagent at a pressure ot Separation agent. 5 kg/cm the solution was sprayed at a.pressure of 100 Water 40 liter kg/cm andboth were brought into contace with each fi l g I Pther y p y g the apparatus shown! I the draw Polystyrene resin powder composed of precisely m spherical particles with excellent fluidity and g 2511. in highest frequency size, the powder having Example 6 apparent specific gravity 0.30 and yield 960 g.

Solution:

Ethylene-vinyl acetate p y 310 2 While spraying the separation agent at a pressure of Tetrahydmfumn 3100 g 3/kg/cm the solution was sprayed at a pressure of 150 Viscosity (55C): 20 cSt Sepawtion agent: 8 l kg/cm and both were brought into contact with each ater 0 iter polynxyethylene alkylether 32 g other by employing the apparatus shown in the draw- Product: mg.

Ethylene-vinyl acetate copolymer powder of precisely spherical particles 20;; in highest Example 10 frequency size. the powder having apparent specific gravity 0.27 and yield 285 g.

Solution:

Styrene-acrylonitril copolymer I000 g 3O Methylethylketone 3800 g While spraying the separation agent at a pressure of Water 200 g 3 kg/cm the solution was sprayed at a pressure of 40 S I If f ltg/cm and both were brought into contact with each 53 i; 35 rim other by employing the apparatus ShOWl'l in the draw- Polyoxyethylene alkylether l4 g Product: ln

g 35 Styrene-acrylonitril copolymer powder composed of precisely spherical particles with Example 7 excellent fluidity and 22y. in highest frequency size, the powder having apparent specific Solution: gravity 0.34 and yield 950 g.

Polyvinyl chloride resin 200 g Tetrahydrofuran 3760 g 40 Water 240 Viscosity: 9 cSt g While spraying the separatlon agent at a pressure of wgg; agent: 50 met 3 kg/cm the solution was sprayed at a pressure of 120 Polyoxyethylene nonylphenol 30 g kg/cm and both were brought into contact with each Product:

Polyvinyl chlorideresin powder of other by employing the apparatus shown in the draw precisely spherical particles with excellent m fluidity and 7 .4. in highest frequency size. the powder having apparent specific gravity 0.31 EXAMPLE 1 l and yield 180 g.

The method of the Example 9 was repeated with spraying pressure for the solution at 5 kg/cm providing Wh1le spraying the separation agent at a pressure of with compressed air and for separation agent at 3 3 kg/cm the solutlon was sprayed at a pressure of 40 kg/cm As a result polystyrene resin powder with 20 a kg/cm and both were brought into contact with each in highest frequency size, apparent specific gravity 029 other by employing the apparatus shown in the drawand yield 960 g was obtained. mg.

EXAMPLE 12 Example 8 The method of the Example 5 was repeated with Solution. spraying pressure for the solution at 6 kg/cm providing Thermoplastic polyurethane resin 100 g with compressed air and for separation agent at 3 Tetrahydrofuran 1640 g 2 water 360 g 0 kg/cm As a result, thermoplastic polyester resin pow- Viscosity: l0 cSt 6 der with 20 p. in highest frequency size. apparent spe- Separation agent:

g l h 20 hm cltlicclgravlty 0.32 and yield 950 g was obtained.

0 yoxyet ylene alkylether 8 g aim: Product:

Thermoplastic polyurethane resin powder 1' A method forprodlilcmg of sphencal pa of precisely spherical particles with excellent tlcles of a synthetlc resm, comprlsmgfluidity and 25p. in highest frequency size. the particles having apparent specific gravity 0.2l and yield g.

a. dissolving a synthetic resin in a volatile organic solvent to form a solution having a viscosity of about 5 to about 200 centistokes:

b. directing a spray of said solution under a pressure of at least 6.5 kg/cm into a chamber to form spherical particles thereof; I I

c. directing into said chamber a spray of a liquid as a separation agent and intersecting said spray ofso- .lution. said resin being insoluble in said liquid separation agent. and the spraying force of said liquid separation agent being about 3 kg/cm" and less than that of said sprayed solution;

d. volatilizing the solvent from the particles of said sprayed solution to form spherical particles of resin powder falling in said chamber, said particles of liquid separation agent serving to separate said powder particles rendered sticky by said volatilization; and,

e. collecting said spherical powder particles in a tank containing said separation agent liquid. from which said powder particles are recovered and dried.

2. A method as claimed in claim I wherein the resin is epoxy resin.

3. A method as claimed in claim 1 wherein the resin is a polyester resin.

4. A method as claimed in claim I wherein the resin is an acetate resin.

5. A method as claimed in claim I wherein the resin is a vinyl chloride resin.

6. A method as claimed in claim 1 wherein the resin is a urethane resin.

7. A method as claimed in claim 1 wherein the resin is a styrene resin.

8. A method as claimed in claim 1 wherein the resin is a acrylonitril resin. 

1. A method for producing a powder of spherical particles of a synthetic resin, comprising: a. dissolving a synthetic resin in a volatile organic solvent to form a solution having a viscosity of about 5 to about 200 centistokes; b. directing a spray of said solution under a pressure of at least 6.5 kg/cm2 into a chamber to form spherical particles thereof; c. directing into said chamber a spray of a liquid as a separation agent and intersecting said spray of solution, said resin being insoluble in said liquid separation agent, and the spraying force of said liquid separation agent being about 3 kg/cm2 and less than that of said sprayed solution; d. volatilizing the solvent from the particles of said sprayed solution to form spherical particles of resin powder falling in said chAmber, said particles of liquid separation agent serving to separate said powder particles rendered sticky by said volatilization; and, e. collecting said spherical powder particles in a tank containing said separation agent liquid, from which said powder particles are recovered and dried.
 1. A METHOD FOR PRODUCING A POWDER OF SPHERICAL PARTICLES OF A SYNTHETIC RESIN, COMPRISING: A. DISSOLVING A SYNTHETIC RESIN IN A VOLATILE ORGANIC SOLVENT TO FORM A SOLUTION HAVING A VISCOSITY OF ABOUT 5 TO ABOUT 200 CENTISTOKES; B. DIRECTING A SPRAY OF SAID SOLUTION UNDER A PRESSURE OF AT LEAST 6.5 KG/CM2 INTO A CHAMBER TO FORM SPHERICAL PARTICLES THEREOF; C. DIRECTING INTO SAID CHAMBER A SPRAY OF A LIQUID AS A SEPARATION AGENT AND INTERSECTING SAID SPRAY OF SOLUTION, SAID RESIN BEING INSOLUBLE IN SAID LIQUID SEPARATION AGENT, AND THE SPRAYING FORCE OF SAID LIQUID SEPARATION AGENT BEING ABOUT 3 KG/CM2 AND LESS THAN THAT OF SAID SPRAYED SOLUTION; D. VOLATILIZING THE SOLVENT FROM THE PARTICLES OF SAID SPRAYED SOLUTION TO FORM SPHERICAL PARTICLES OF RESIN POWDER FALLING IN SAID CHAMBER, SAID PARTICLES OF LIQUID SEPARATION AGENT SERVING TO SEPARATE SAID POWDER PARTICLES RENDERED STICKY BY SAID VOLATILIZATION; AND, E. COLLECTING SAID SPHERICAL POWDER PARTICLES IN A TANK CONTAINING SAID SEPARATION AGENT LIQUID, FROM WHICH SAID POWDER PARTICLES ARE RECOVERED AND DRIED.
 2. A method as claimed in claim 1 wherein the resin is epoxy resin.
 3. A method as claimed in claim 1 wherein the resin is a polyester resin.
 4. A method as claimed in claim 1 wherein the resin is an acetate resin.
 5. A method as claimed in claim 1 wherein the resin is a vinyl chloride resin.
 6. A method as claimed in claim 1 wherein the resin is a urethane resin.
 7. A method as claimed in claim 1 wherein the resin is a styrene resin. 